CN112320812A - Method for synthesizing white potassic mica by using red mixed clay mineral - Google Patents
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- C01B33/00—Silicon; Compounds thereof
- C01B33/20—Silicates
- C01B33/36—Silicates having base-exchange properties but not having molecular sieve properties
- C01B33/38—Layered base-exchange silicates, e.g. clays, micas or alkali metal silicates of kenyaite or magadiite type
- C01B33/42—Micas ; Interstratified clay-mica products
Abstract
The application provides a method for synthesizing white potassic mica by using red mixed clay minerals, belonging to the technical field of deep processing of non-metallic ores and synthesis of nano materials. The method utilizes simple one-step hydrothermal reaction to convert red mixed clay into white potassium mica, thereby realizing the white conversion of a red mineral structure and the mineral structure conversion. The product has good batch stability, uniform granularity and simple preparation process, can be potentially used in a plurality of aspects such as lubricating materials, high polymer material fillers, coatings, lithium ion battery diaphragm coatings, catalyst carriers, hybrid pigments, antibacterial material matrixes, heavy metals, dyes, antibiotic adsorbents and the like, is beneficial to expanding the application field of red mixed clay minerals, and is also beneficial to realizing high-valued utilization of local characteristic dominant resources.
Description
Technical Field
The invention relates to a method for synthesizing white potassic mica by using red mixed clay minerals, belonging to the technical field of deep processing of non-metallic ores and synthesis of nano materials.
Background
The clay mineral is a special non-metallic mineral formed naturally by nature, not only has unique crystal structure and excellent colloid, adsorption, carrier and reinforcement performance, but also has incomparable advantages of artificial synthetic materials from nature, abundant reserves, environmental friendliness and the like. Therefore, clay minerals, which are essential and important basic materials, play an extremely important role in various fields of agriculture, chemical industry, environmental protection, building materials, life and health, new materials and other national economy.
The clay mineral is a dominant and characteristic mineral resource in China, and the prospect reserves are extremely rich, but the greater part of the clay mineral is typical lake-phase or sea-phase sedimentary mineral, the isomorphous substitution phenomenon of Fe (III) can occur in the process of mineralization, and a plurality of associated minerals are formed at the same time, so that the composition of the minerals is complex and the minerals are in brick red. The red clay minerals with huge reserves in autonomous regions of Mongolia autonomous regions and Gansu provinces in China are the most representative, the prospect reserves reach more than 30 hundred million tons, and the hidden potential application value is unlimited. The mineral composition analysis result shows that the red clay consists of clay minerals such as attapulgite, illite, chlorite and illite mixed-layer clay and symbiotic or associated minerals such as calcite, dolomite, hematite and quartz. Due to the complex composition, dark color and poor performance of the clay minerals, products with high added values are difficult to develop by using the prior art method, so that the resource utilization rate and the market competitiveness of the products are low, and the high-efficiency and high-value development and utilization of the dominant mineral resources in China are restricted.
In the related art, a method for improving the content of attapulgite in clay by a purification method is commonly used to improve the service performance of the clay. Chinese patent CN102874826A discloses a method for purifying attapulgite clay, which comprises the steps of dispersing attapulgite clay in water for pulping, adding an activating agent for activation, adding acid for impurity removal, aging, performing gravity settling, performing multiple centrifugal separation, and finally obtaining purified attapulgite. Chinese patent CN103738975A discloses a purification method of attapulgite clay, which adopts the steps of pulping, adding an activator, aging, settling, separating and the like to improve the purity of the attapulgite clay. Although the purification treatment can reduce the content of miscellaneous minerals to a certain extent, the purity of the attapulgite is improved, and the service performance is improved. However, the red mixed clay mineral has complex mineral composition and low content of main components, so that the purification process is complex, the cost is high, the water and energy consumption is high, and the use of a chemical dispersing agent for purification can cause environmental pollution. In addition, for red clay minerals, even though the purity can be improved moderately by purification, the red color of the minerals cannot be eliminated. Therefore, the use performance of the mixed clay mineral is difficult to be obviously improved by using the conventional purification and modification method.
Since the clay mineral components are composed of silicon-oxygen tetrahedrons and metal-oxygen octahedrons, the clay mineral components are transformed into other types of minerals or materials through crystal form recombination under specific reaction conditions. Chinese patent CN103708483A discloses a method for preparing attapulgite montmorillonite by in-situ crystal transformation, and the method for recombining an attapulgite structure into a novel mineral structure remarkably improves the adsorption performance; chinese patent CN104445240A discloses a method for preparing an organic mixed-dimension nano material in situ by attapulgite, and prepares an adsorption material with excellent performance by crystal transformation of the attapulgite. Chinese patent CN106315605B discloses a method for preparing tobermorite from low-grade attapulgite clay under strong alkaline reaction conditions. Chinese patent CN105664843B discloses a method for preparing micro-nano mesoporous adsorption microspheres by using attapulgite clay, wherein the adsorption performance of the attapulgite is improved by introducing magnesium silicate, but the obtained product is still red. These research and invention results show that the structural transformation of mixed clay minerals by controlling reaction conditions is a new way for effective utilization thereof.
Potassium mica is a monoclinic layered silicate with a chemical composition of KAl2(AlSi3O10) (OH)2, belonging to the mica group of minerals. The crystal is in a pseudo hexagonal flake shape, an aggregate flake shape or a scaly shape, and has glass luster, hardness of 2.5-3 and density of 2.76-3.10 g/cm 3. Has high electric insulation, heat resistance and good mechanical property. Because the potassium mica has the characteristics of insulation, high temperature resistance, luster, physical and chemical property stability, heat insulation, elasticity, toughness and the like, the potassium mica is widely applied to the aspects of daily chemical industry, ceramics, paint, plastic and rubber additives, building materials, lubricating materials, welding rod coating protective layers, high polymer insulating materials, papermaking, asphalt paper, pearlescent pigments, flame retardant fillers and the like. Due to the specific two-dimensional layered structure of the potassium mica, the potassium mica can be intercalated or peeled at a high temperature to form a two-dimensional nano material (Chinese patent CN104445235A), and the dispersibility of the powder can be improved through surface modification to prepare the ultrafine mica powder (Chinese patent CN 102732069B). At present, researches and application development on potassium mica mainly focus on preparing composite Materials (Chinese patent CN 102492312B; CN 101880350A; CN 101844915A; CN 109320990A; CN 111297710A; CN105754075A), antibacterial Materials (Chinese patent CN102660114A), concrete antifreezes (Chinese patent CN107098615A), adsorbing Materials (Journal of Hazardous Materials 2021,401:123249) and the like. In recent years, there are related patent reports on the preparation of nano kaolinite (Chinese patent CN107572542A) by using potassium mica powder and the synthesis of nano potassium mica (Chinese patent CN107522208A) by using kaliophilite powder (KAlSiO4),
however, the white potassium mica with better whiteness is prepared by the one-pot reaction of the red mixed clay mineral, so far, no relevant research report exists, and no prior case of industrial application exists.
Disclosure of Invention
The application aims to provide a method for synthesizing white potassium mica by using red mixed clay minerals, which converts the one-pot hydrothermal reaction of the red mixed clay minerals into the white potassium mica by adjusting the raw material proportion and the reaction conditions, synchronously realizes the white conversion and the crystal phase conversion of the red minerals, and provides a new idea for the high-value utilization of the red mixed clay resources with abundant reserves in China.
The application provides a method for synthesizing white potassic mica by using red mixed clay minerals, which comprises the following steps:
(1) crushing the red mixed clay mineral, sieving the crushed red mixed clay mineral with a 200-mesh sieve, fully mixing the red mixed clay mineral with an aqueous solution containing 5% of hydrogen peroxide and 2.5% of nitric acid to ensure that the water content in the mineral powder reaches 20-35%, and then sequentially carrying out three-roll extrusion grinding treatment for 2 times and air plasma ball milling treatment for 30-60 min to obtain an activated solid precursor.
(2) Dispersing the solid precursor into a water solution of complexing acid according to a solid-to-liquid ratio of 1:9, then adding an auxiliary agent glutamic acid accounting for 0.025-0.1% of the mass of the clay mineral, carrying out ultrasonic treatment for 10 minutes, mechanically stirring to fully and uniformly mix the mixture, and carrying out hydrothermal reaction for 2-11.5 hours under certain pressure and at a temperature of 140-208 ℃;
(3) and after the reaction kettle is naturally cooled to room temperature, carrying out centrifugal separation, washing, drying and crushing on the solid reaction product to obtain a white potassium mica product.
In one possible embodiment, the red mixed clay mineral comprises attapulgite, illite, chlorite, illite-smectite mixed-layer clay, calcite, dolomite, hematite.
In a possible embodiment, the discharge voltage of the air plasma ball milling treatment is 8-12 kV, the power of a discharge power supply is 1.0-2.5 KW, and the rotating speed is 950-1450 rpm.
In one possible embodiment, the complexing acid is at least one of oxalic acid, ethylenediaminetetraacetic acid, and sulfamic acid.
In one possible embodiment, the concentration of the complexing acid aqueous solution is 0.20 to 1.80 mol/L.
In one possible embodiment, the hydrothermal reaction pressure is 3 to 5 MPa.
The method for synthesizing white potassium mica by using red mixed clay minerals has the beneficial effects that: the red mixed clay is converted into white potassium mica by a simple one-step hydrothermal reaction, so that the white conversion of a red mineral structure is realized, and the mineral structure conversion is also realized. The product has good batch stability, uniform granularity and simple preparation process, can be potentially used in various aspects such as high polymer material fillers, lubricating materials, coatings, lithium ion battery diaphragm coatings, catalyst carriers, hybrid pigments, antibacterial material matrixes, heavy metals, dyes, antibiotic adsorbents and the like, is favorable for expanding the application field of red mixed clay minerals, and is also favorable for realizing high-valued utilization of local characteristic dominant resources.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present application, the drawings needed to be used in the embodiments are briefly described below, it should be understood that the following drawings only illustrate some embodiments of the present application and therefore should not be considered as limiting the scope, and for those skilled in the art, other related drawings can be obtained from the drawings without inventive efforts and also belong to the protection scope of the present application.
FIG. 1 is a digital photograph of red mixed clay and white potassic mica product prepared by the process of the present invention;
FIG. 2 is an XRD spectrum of a red mixed clay and a white potassic mica product prepared by the process of the invention;
fig. 3 is a TEM image of red mixed clay and white potassic mica product prepared by the process described in example 2 of the present invention.
Detailed Description
The embodiment of the application provides a method for synthesizing white potassic mica by using red mixed clay minerals, which comprises the following steps
(1) Crushing the red mixed clay mineral, sieving the crushed red mixed clay mineral with a 200-mesh sieve, fully mixing the red mixed clay mineral with an aqueous solution containing 5% of hydrogen peroxide and 2.5% of nitric acid to ensure that the water content in the mineral powder reaches 20-35%, and then sequentially carrying out three-roll extrusion grinding treatment for 2 times and air plasma ball milling treatment for 30-60 min to obtain an activated solid precursor.
Optionally, the red mixed clay mineral mainly contains attapulgite (content 23.2-37.3%), illite (content 9.6-14.5%), chlorite (content 7.6-12.1%), illite mixed layer clay (content 3.1-6.2%), calcite (content 7.9-18.2%), dolomite (content 1.5-2.8%), and hematite (content 3.2-4.9%).
Further, the discharge voltage during the air plasma ball milling treatment is 8-12 kV, the power of a discharge power supply is 1.0-2.5 KW, and the rotating speed is 950-1450 rpm.
(2) Dispersing the solid precursor into a water solution of complexing acid according to a solid-to-liquid ratio of 1:9, then adding an auxiliary agent glutamic acid accounting for 0.025-0.1% of the mass of the clay mineral, carrying out ultrasonic treatment for 10 minutes, mechanically stirring to fully and uniformly mix the precursor and the glutamic acid, and carrying out hydrothermal reaction for 2-11.5 hours under certain pressure and at a temperature of 140-208 ℃.
Optionally, the complexing acid is at least one of oxalic acid, ethylenediaminetetraacetic acid, and sulfamic acid. The concentration of the complexing acid aqueous solution is 0.20-1.80 mol/L.
Wherein the hydrothermal reaction pressure is 3-5 MPa.
(3) And after the reaction kettle is naturally cooled to room temperature, carrying out centrifugal separation, washing, drying and crushing on the solid reaction product to obtain a white potassium mica product.
The application provides a method for synthesizing white potassium mica by using red mixed clay minerals, which converts the red mixed clay into the white potassium mica by simple one-step hydrothermal reaction, thereby realizing the white conversion of a red mineral structure and the mineral structure conversion. The product has good batch stability, uniform granularity and simple preparation process, can be potentially used in various aspects such as high polymer material fillers, lubricating materials, coatings, lithium ion battery diaphragm coatings, catalyst carriers, hybrid pigments, antibacterial material matrixes, heavy metals, dyes, antibiotic adsorbents and the like, is favorable for expanding the application field of red mixed clay minerals, and is also favorable for realizing high-valued utilization of local characteristic dominant resources.
In order to make the objects, technical solutions and advantages of the embodiments of the present application clearer, the technical solutions of the embodiments of the present application will be clearly and completely described below. The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products available commercially.
Example 1:
100kg of red mixed clay mineral (containing 37.3% of attapulgite, 9.6% of illite, 12.1% of chlorite, 6.2% of illite mixed layer clay, 7.9% of calcite, 2.8% of dolomite and 4.9% of hematite) is crushed and sieved by a 200-mesh sieve, 25kg of aqueous solution containing 5% (mass fraction) of hydrogen peroxide and 2.5% (mass fraction) of nitric acid is sprayed on the red mixed clay mineral, and the mixture is stirred and mixed uniformly. Then the wetted mineral powder is subjected to three-roll extrusion grinding for 2 times, and then is subjected to air plasma ball milling (discharge voltage: 12 kV; discharge power: 2.5KW, rotation speed: 950rpm) for 30min, so as to obtain an activated solid precursor. Dispersing the solid precursor into 1.80mol/L sulfamic acid aqueous solution according to the solid-to-liquid ratio of 1:9, then adding 25g of glutamic acid as an auxiliary agent, carrying out ultrasonic treatment for 10 minutes, then carrying out mechanical stirring to fully and uniformly mix the glutamic acid and the amino sulfonic acid, and then carrying out hydrothermal reaction for 11.5 hours under the conditions of the pressure of 5MPa and the temperature of 208 ℃. After the reaction kettle is naturally cooled to room temperature, the solid reaction product is centrifugally separated, washed, dried and crushed to obtain a white potassium mica product (the number is MVT-1).
Example 2:
100kg of red mixed clay mineral (containing 35.2% of attapulgite, 14.5% of illite, 7.6% of chlorite, 3.1% of illite mixed layer clay, 18.2% of calcite, 1.5% of dolomite and 3.2% of hematite) is crushed and sieved by a 200-mesh sieve, 53.85kg of aqueous solution containing 5% (mass fraction) of hydrogen peroxide and 2.5% (mass fraction) of nitric acid is sprayed on the red mixed clay mineral, and the mixture is stirred and mixed uniformly. And then carrying out three-roll extrusion grinding treatment on the wetted mineral powder for 2 times, and then carrying out air plasma ball milling (the discharge voltage is 8kV, the power of a discharge power supply is 1.0KW, and the rotating speed is 1450rpm) for 60min to obtain an activated solid precursor. Dispersing the solid precursor into 0.20mol/L ethylene diamine tetraacetic acid aqueous solution according to the solid-liquid ratio of 1:9, then adding 100g of glutamic acid as a reaction auxiliary agent, carrying out ultrasonic treatment for 10 minutes, then carrying out mechanical stirring to fully and uniformly mix the glutamic acid and the reaction auxiliary agent, and carrying out hydrothermal reaction for 2 hours under the conditions of the pressure of 3MPa and the temperature of 208 ℃. After the reaction kettle is naturally cooled to room temperature, the solid reaction product is centrifugally separated, washed, dried and crushed to obtain a white potassium mica product (the number is MVT-2).
Example 3:
100kg of red mixed clay mineral (containing 23.2% of attapulgite, 14.5% of illite, 12.0% of chlorite, 6.1% of illite mixed layer clay, 16.1% of calcite, 2.6% of dolomite and 4.7% of hematite) is crushed and sieved by a 200-mesh sieve, 35kg of an aqueous solution containing 5% (mass fraction) of hydrogen peroxide and 2.5% (mass fraction) of nitric acid is sprayed on the crushed mixed clay mineral, and then the crushed mixed clay mineral and the aqueous solution are fully mixed. And then carrying out three-roll extrusion grinding treatment on the wetted powder for 2 times, and then carrying out air plasma ball milling (the discharge voltage is 10kV, the power of a discharge power supply is 2KW, and the rotating speed is 1200rpm) for 40min to obtain an activated solid precursor. Dispersing the solid precursor into a mixed acid water solution containing 0.8mol/L oxalic acid and 0.8mol/L ethylene diamine tetraacetic acid according to a solid-to-liquid ratio of 1:9, then adding 50g of auxiliary glutamic acid, carrying out ultrasonic treatment for 10 minutes, mechanically stirring to fully and uniformly mix the glutamic acid and the auxiliary glutamic acid, and carrying out hydrothermal reaction for 8 hours under the conditions of a pressure of 3MPa and a temperature of 180 ℃. After the reaction kettle is naturally cooled to room temperature, the solid reaction product is centrifugally separated, washed, dried and crushed to obtain a white potassium mica product (the number is MVT-3).
Example 4:
100kg of red mixed clay mineral (containing 37.3% of attapulgite, 9.6% of illite, 12.1% of chlorite, 6.2% of illite mixed layer clay, 7.9% of calcite, 2.8% of dolomite and 4.9% of hematite) is crushed and sieved by a 200-mesh sieve, and 33kg of aqueous solution containing 5% (mass fraction) of hydrogen peroxide and 2.5% (mass fraction) of nitric acid is sprayed on the crushed material, and the mixture is stirred and mixed uniformly. And then carrying out three-roll extrusion grinding treatment on the wetted powder for 2 times, and then carrying out air plasma ball milling (the discharge voltage is 10kV, the power of a discharge power supply is 2KW, and the rotating speed is 1000rpm) for 50min to obtain an activated solid precursor. Dispersing the solid precursor into 1.5mol/L oxalic acid aqueous solution according to the solid-to-liquid ratio of 1:9, then adding 45g of auxiliary agent glutamic acid, carrying out ultrasonic treatment for 10 minutes, mechanically stirring to fully and uniformly mix the precursor, and carrying out hydrothermal reaction for 10 hours under the conditions of the pressure of 4MPa and the temperature of 200 ℃. After the reaction kettle is naturally cooled to room temperature, the solid reaction product is centrifugally separated, washed, dried and crushed to obtain a white potassium mica product (the number is MVT-4).
Example 5:
100kg of red mixed clay mineral (containing 37.3% of attapulgite, 9.6% of illite, 12.1% of chlorite, 6.2% of illite mixed layer clay, 7.9% of calcite, 2.8% of dolomite and 4.9% of hematite) is crushed and sieved by a 200-mesh sieve, 45kg of aqueous solution containing 5% (mass fraction) of hydrogen peroxide and 2.5% (mass fraction) of nitric acid is sprayed on the crushed material, and the mixture is stirred and mixed uniformly. And then carrying out three-roll extrusion grinding treatment on the wetted powder for 2 times, and then carrying out air plasma ball milling (discharge voltage is 12kV, power of a discharge power supply is 1.5KW, and rotating speed is 1350rpm) for 60min to obtain an activated solid precursor. Dispersing the solid precursor into a mixed acid aqueous solution containing 0.5mol/L sulfamic acid and 1.0mol/L oxalic acid according to the solid-to-liquid ratio of 1:9, then adding 30g of auxiliary agent glutamic acid, carrying out ultrasonic treatment for 10 minutes, mechanically stirring to fully and uniformly mix the precursor, and carrying out hydrothermal reaction for 6 hours under the conditions of certain pressure and 190 ℃. After the reaction kettle is naturally cooled to room temperature, the solid reaction product is centrifugally separated, washed, dried and crushed to obtain a white potassium mica product (the number is MVT-5).
Structure and properties of potassium mica: as can be seen from FIG. 1, the potassium micas prepared by the process described in examples 1-5 are white in color and the CIE-lab color values are shown in Table 1. The L value (representing the brightness value of the sample) of the red mixed clay is only 62.212, and after the red mixed clay is treated by the process disclosed by the invention, the L value of the sample is increased to 86.464-86.900; meanwhile, the value a (representing the red tone) is reduced from 13.437 to 0.011-0.243, which shows that the red color of the clay mineral is changed into white color after the clay mineral is treated by the process of the invention. Analyzing the structure and morphology of the potassic mica product by X-ray powder diffraction (XRD) and Scanning Electron Microscope (SEM); fig. 2 is XRD patterns of clay mineral used in example 1 and prepared potassic mica, and it can be seen from fig. 2 that after the red mixed clay is treated by the method of the present invention, characteristic diffraction peaks of attapulgite at 2 θ -8.47 ° (110 crystal face) and 2 θ -12.48 ° (200 crystal face), characteristic diffraction peaks of chlorite at 2 θ -6.20 ° and characteristic diffraction peaks of illite at 2 θ -8.87 ° disappear, and characteristic diffraction peaks of 002 crystal face and 004 crystal face of potassic mica appear at 2 θ -8.90 ° and 17.82 ° respectively, which proves that the main product obtained after the red clay mineral is treated by the process of the present invention is potassic mica; as can be seen from FIG. 3, after the treatment by the method of the present invention, the attapulgite nanorods and iron oxide and other impurity particles in the red mixed clay disappear, and a large amount of lamellar substances appear, indicating that the obtained product is lamellar potassium mica.
TABLE 1 CIE color values of Red Clay blends and white potassic mica products prepared by the Process according to the invention
The embodiments described above are some, but not all embodiments of the present application. The detailed description of the embodiments of the present application is not intended to limit the scope of the claimed application, but is merely representative of selected embodiments of the application. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present application.
Claims (6)
1. A method for synthesizing white potassic mica by using red mixed clay minerals is characterized in that: comprises the following steps
(1) Crushing the red mixed clay mineral, sieving the crushed red mixed clay mineral with a 200-mesh sieve, fully mixing the red mixed clay mineral with an aqueous solution containing 5% of hydrogen peroxide and 2.5% of nitric acid to ensure that the water content in the mineral powder reaches 20-35%, and then sequentially carrying out three-roll extrusion grinding treatment for 2 times and air plasma ball milling treatment for 30-60 min to obtain an activated solid precursor.
(2) Dispersing the solid precursor into a water solution of complexing acid according to a solid-to-liquid ratio of 1:9, then adding an auxiliary agent glutamic acid accounting for 0.025-0.1% of the mass of the clay mineral, carrying out ultrasonic treatment for 10 minutes, mechanically stirring to fully and uniformly mix the mixture, and carrying out hydrothermal reaction for 2-11.5 hours under certain pressure and at a temperature of 140-208 ℃;
(3) and after the reaction kettle is naturally cooled to room temperature, carrying out centrifugal separation, washing, drying and crushing on the solid reaction product to obtain a white potassium mica product.
2. The method for synthesizing white potassium mica by using red mixed clay minerals, according to claim 1, wherein the method comprises the following steps: the red mixed clay mineral comprises attapulgite, illite, chlorite, illite mixed-layer clay, calcite, dolomite and hematite.
3. The method for synthesizing white potassium mica by using red mixed clay minerals, according to claim 1, wherein the method comprises the following steps: the discharge voltage during the air plasma ball milling treatment is 8-12 kV, the power of a discharge power supply is 1.0-2.5 KW, and the rotating speed is 950-1450 rpm.
4. The method for synthesizing white potassium mica by using red mixed clay minerals, according to claim 1, wherein the method comprises the following steps: the complexing acid is at least one of oxalic acid, ethylene diamine tetraacetic acid and sulfamic acid.
5. The method for synthesizing white potassium mica by using red mixed clay minerals, according to claim 1, wherein the method comprises the following steps: the concentration of the complexing acid aqueous solution is 0.20-1.80 mol/L.
6. The method for synthesizing white potassium mica by using red mixed clay minerals, according to claim 1, wherein the method comprises the following steps: the hydrothermal reaction pressure is 3-5 MPa.
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